Crystal structure and molecular geometry of a square-pyramidal platinum(II) complex [{2,6-(Me2NCH2)2C6H3}Pt(.mu.-{(p-tol)NC(H)N(i-Pr)})HgBrCl] containing a PtII-to-HgII donor bond

A highly sensitive and selective method using liquid chromatography coupled with tandem mass spectrometry (LC/MS/MS) was developed and validated for the measurement of three antiretroviral agents, efavirenz, lopinavir and ritonavir, in human hair. Hair samples from adherent HIV-infected patients on antiretroviral therapies were cut into about 1 mm length segments and drugs were extracted by first shaking the samples with methanol in a 37°C water bath overnight (>14 h), followed by methyl tert-butyl ether/ethyl acetate (1:1) extraction under weak alkaline conditions. The extracted lopinavir and ritonavir were separated by reversed-phase chromatography and detected by tandem mass spectrometry in electrospray positive ionization mode with multiple reaction monitoring (MRM), while efavirenz was monitored in negative ionization MRM mode. This method was validated from 0.01 to 4.0 ng/mg hair for ritonavir and 0.05–20 ng/mg hair for lopinavir and efavirenz by using 2 mg of a human hair sample. The interday and intraday assay precision (coefficients of variation, CV) for spiked quality control (QC) samples at low, medium and high concentrations were within 15% and accuracy ranged from 89% to 110%. Assay reproducibility was also demonstrated by analysis of incurred hair QC samples (CV <14%). No significant matrix ionization suppression was observed. This developed method allowed for the monitoring of these target medications in the hair samples of HIV-infected women on antiretroviral therapy in an observational study using small amounts of hair.

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“… Molecular structure of a heterobimetallic pincer complex containing a direct platinum–mercury bond 53a…”

Section: New Materials Propertiesmentioning

confidence: 99%

Sensitive analysis of anti‐HIV drugs, efavirenz, lopinavir and ritonavir, in human hair by liquid chromatography coupled with tandem mass spectrometry

Huang

Gandhi

Greenblatt

et al. 2008

Rapid Comm Mass Spectrometry

116

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“…In yellow orthorhombic Pt(II)Hg(II) dimer (van der Ploeg et al, 1980(van der Ploeg et al, , 1982a, two units Pt( η 2 -danp) 2 and Hg( η 1 -ac) are connected by a direct Pt-Hg bond [2.513(1) Å ] as well as acetate ligand which serve as a bridge via O atoms of the carboxylate group. The Pt(II) is hexa-coordinated (PtN 2 C 2 PHg) and Hg(II) three-(HgO 2 Pt) of T shape.…”

Section: Ptm (M = = Zn CD or Hg) Complexesmentioning

confidence: 99%

Structural characterisation of heterometallic platinum complexes with non-transition metals. Part I: heterodimeric complexes

Melnik

Mikuš

2012

Main Group Metal Chemistry

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This review covers 90 heterodimeric Pt complexes with non-transition metals. There are 13 non-transition metals (Ge, Sn, Pb, Ga, In, Tl, Sb, Zn, Cd, Hg, Na, K and Ca). These dimers can be divided into three groups, the first in which only a direct Pt-M bond connects respective units (59%); the second in which in additon to a direct Pt-M bond a ligand/s serves as bridge/s (33%); and the third one in which two respective units are held together via bridge/s ligand/s. The mean Pt-M bond distance elongates in the sequence: 2.425 Å (M = Ge) < 2.559 Å (Sb) < 2.601 Å (In) < 2.625 Å (Cd) < 2.657 Å (Hg) < 2.663 Å (Sn) < 2.670 Å (Pb) < 2.674 Å (Tl) < 2.760 Å (Zn) < 2.960 Å (Ca). The Pt atom has oxidation numbers 0, + 2 (most common) and + 4, and the M atoms have + 1, + 2 (most common), + 3 and + 4. The Pt coordination geometrics include square planar (most common), trigonal bi pyramidal, pseudo-octahedral Pt(IV). There are examples which contain two independent dimers (distortion isomers). Factors affecting bond distances and angles are discussed and some ambiguities in coordination poly hedra are outlined.

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“… Molekülstruktur eines Heterodimetall‐Pinzetten‐Komplexes mit einer direkten Platin‐Quecksilber‐Bindung 53a…”

Section: Neue Materialeigenschaftenunclassified

Metallorganische Pinzetten-Komplexe von Elementen der Platingruppe: Sensoren, Schalter und Katalysatoren

2001

Self Cite

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Seit den ersten Berichten über Übergangsmetallkomplexe mit Pinzetten‐Liganden in den späten siebziger Jahren haben diese Systeme wegen der ungewöhnlichen Eigenschaften, die das Metallzentrum durch den Pinzetten‐Liganden erhält, zunehmendes Interesse hervorgerufen. Typischerweise enthält ein solcher Ligand einen anionischen Arenring, der an beiden ortho‐Positionen mit Heteroatomsubstituenten, z. B. CH2NR2, CH2PR2 oder CH2SR, substituiert ist. Die Heteroatomsubstituenten koordinieren im Allgemeinen ebenfalls an das Metallzentrum und unterstützen daher die M‐C‐σ‐Bindung. Häufig führt dies zu einer dreizähnigen meridionalen Koordination, bei der zwei Metallacyclen gebildet werden, die sich die M‐C‐Bindung teilen. Detaillierte Studien zur Bildung und zu den Eigenschaften einer großen Vielfalt an Pinzetten‐Komplexen von Elementen der Platingruppe führten sowohl zu einem grundlegenden Verständnis vieler Reaktionen der Organometallchemie als auch zu einer Reihe neuer Anwendungen. Die Entdeckung von Katalysatoren für die Alkandehydrierung, die Aufklärung der Mechanismen bestimmter Basisreaktionen (z. B. der C‐C‐Aktivierung) sowie die Entwicklung der ersten wiederverwendbaren Metallodendrimere als Katalysatoren in der homogenen Katalyse und kristalliner Schalter zur Materialveredelung sind nur einige der vielen Höhepunkte, die aus den vielfältigen Untersuchungen hervorgegangen sind. In dieser Übersicht werden zum einen die Synthesemethoden besprochen, die zurzeit für die Herstellung von Komplexen aus Elementen der Platingruppe und Pinzetten‐Liganden bekannt sind. Zum anderen werden vor allem Anwendungen von Pinzetten‐Komplexen in den Materialwissenschaften, wie die Entwicklung und Veredelung von Sensoren, Schaltern und Katalysatoren, diskutiert.

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Crystal structure and molecular geometry of a square-pyramidal platinum(II) complex [{2,6-(Me2NCH2)2C6H3}Pt(.mu.-{(p-tol)NC(H)N(i-Pr)})HgBrCl] containing a PtII-to-HgII donor bond

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Sensitive analysis of anti‐HIV drugs, efavirenz, lopinavir and ritonavir, in human hair by liquid chromatography coupled with tandem mass spectrometry

Sensitive analysis of anti‐HIV drugs, efavirenz, lopinavir and ritonavir, in human hair by liquid chromatography coupled with tandem mass spectrometry

Structural characterisation of heterometallic platinum complexes with non-transition metals. Part I: heterodimeric complexes

Metallorganische Pinzetten-Komplexe von Elementen der Platingruppe: Sensoren, Schalter und Katalysatoren

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